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Sulfated Zirconia on Dendritic Fibrous Nanosilica (DFNS): An Efficient Catalyst for the Conversion of Furfuryl Alcohol to 2-Ethylhexyl Levulinate
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DOI：10.1021/acs.energyfuels.5c05633.png)
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Abstract
En 中文
The synthesis of alkyl levulinates (ALs) and their derivatives using biomass-derived feedstocks and green chemistry principles remains a major challenge in sustainable catalysis. In this work, the conversion of furfuryl alcohol (FFA) into 2-ethylhexyl levulinate (2-EHL)─a valuable biobased fuel additive─was investigated using 2-ethylhexanol (2-EH) as both solvent and reactant. A highly efficient solid superacid catalyst, sulfated zirconia supported on dendritic fibrous nanosilica (SO4/ZrO2/DFNS(x)), was designed and optimized. The effects of catalyst loading, reaction temperature, reaction time, reactant-to-solvent ratio, and substrate type were systematically studied to determine the optimal reaction conditions and active site configuration. Under the optimized conditions (20 mg catalyst, 1 mL FFA, 5 mL 2-EH, 140 °C, 4 h), the SO4/ZrO2/DFNS(Opt) catalyst achieved an outstanding 89.7% yield of 2-EHL with complete FFA conversion, minimal humin formation, and maintaining good reusability (79.1% yield after three cycles). The superior catalytic performance was attributed to the predominance of the tetragonal ZrO2 crystalline phase, as confirmed by structural analysis indicating a higher density of accessible active sites. Moreover, using levulinic acid (LA) as a substrate under similar conditions resulted in a 100% yield, confirming the high catalytic activity. The proposed reaction mechanism showed strong agreement with the experimental results. The synthesized 2-EHL was confirmed by FTIR, NMR, and GC–MS analyses, while the catalyst structure and properties were comprehensively characterized using FTIR, BET, XRD, TGA/DTG, ICP-OES, TEM, FE-SEM, and EDS mapping.
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